CN106185964A - A kind of preparation method of super insulating material silicon dioxide - Google Patents
A kind of preparation method of super insulating material silicon dioxide Download PDFInfo
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Abstract
The present invention provides the preparation method of the super insulating material silicon dioxide that a kind of nanoporous structure do not caves in, including: after silica slurry is frozen into solid, carry out vacuum lyophilization, obtain silicon-dioxide powdery, then silicon-dioxide powdery is heated to 130～180 DEG C, stirring while adding silazane, obtaining super insulating material silicon dioxide.The beneficial effects of the present invention is: use cryodesiccated mode, make the filter cake of the silicon dioxide of synthesis, through being frozen into solid, evacuation at low temperatures, obtains water in making silicon dioxide micropore and is directly risen Huawei's vaporous water by solid, vaporous water is removed, it is by ice distillation dehydration during due to removing water, there is not the surface tension of water, when making super insulating material silicon dioxide be dried, nanometer micropore does not caves in, and has good insulation effect；Use silazane that silica product is carried out surface modification, obtain hydrophobic silicon dioxide, solve the phenomenon of nanometer micropore silicon dioxide water suction.
Description
Technical field
The present invention relates to super insulating material, the preparation side of a kind of super insulating material silicon dioxide
Method.
Background technology
Super insulating material silicon dioxide refers under the conditions of predetermined use, and its heat conductivity is less than " empty without convection current
Gas " adiabator of heat conductivity 0.023W/m k.Nano-porous super thermal insulation material silicon dioxide should be provided simultaneously with following several
Individual feature: the almost all of aperture of nano-porous super thermal insulation material silicon dioxide all should be at below 60nm.In adiabator
Pore size is the main factor of heat-insulating property, and therefore, the only most pore sizes in adiabator are less than 60nm
Time, just calculate the category entering nano material.In material, the pore size of major part (more than 90%) all answers < 40nm.According to dividing
Son motion and collision theory, the heat transmission of gas is mainly the molecule of the fair speed by high temperature side and the relatively low of low temperature side
The molecule of speed mutually collides and carries out, due in air the free path of main component nitrogen and oxygen all at about 70nm,
SiO in Nanometer-porous2When the pore size that microgranule is constituted is less than this critical dimension, material internal eliminates the need for
Convection current, has inherently cut off the conduction of heat of gas molecule, thus can obtain ratio " without the heat conductivity that convected air is lower.
High pore volume silicon dioxide should have the lowest bulk density.There is substantial amounts of micropore in the silicon dioxide of high pore volume, tool
There is low bulk density 100Kg/m3。
Super insulating material silicon dioxide, at a temperature of the use of room temperature and setting, all should have than " without convected air "
Lower heat conductivity.Heat conductivity is to weigh the leading indicator that adiabator performance is good and bad.The air that remains static and
The heat conductivity of major part gas is the lowest, but due to their convection current performance, and the transparency to infra-red radiation, determine
They cannot be used alone as adiabator.For this reason, it may be necessary to use some solid materials to limit their convection current performance and thoroughly
Infrared ray performance.But, almost all of solid material all has the heat conductivity more much bigger than still air.Thus, in order to
Reducing the conduction of heat of solid material to greatest extent, the solid thin-walled as gas shield should be the thinnest.Simultaneously, it is contemplated that by solid
Between the size in space be limited to nanometer scale, then conduction and the convection current of gas will be substantially achieved control, this kind of adiabator
Heat conductivity will be less than static air.
Super insulating material silicon dioxide has preferable resistance to elevated temperatures.
But in the preparation technology of existing super insulating material silicon dioxide, it is primarily present following problem:
Owing to existing silicon dioxide synthesis technique is to synthesize in aqueous, have to be dehydrated when dry.Due to all
Act on liquid surface, make the existence of the surface tension of liquid of the power that liquid surface area reduces, surface tension 72.8mN/m of water
(20 DEG C), γ=ρ ghr/ (2cos θ), nanometer micropore is made micropore cave in by capillary impact, hardly results in aperture and concentrates
Degree reach more than 90% and average pore size at the silicon dioxide of the big pore volume of micropore of below 40nm.
Nanometer micropore silicon dioxide water absorption is big, if when using, water entrance can cause nanoporous structure to cave in, the leading of water
Hot coefficient, much larger than the mesoporous silica of nanometer, causes super effect heat insulation material silicon dioxide effect to be deteriorated.
Summary of the invention
The technical problem to be solved is: the super insulating material providing a kind of nanoporous structure not cave in is used
The preparation method of silicon dioxide.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: a kind of super insulating material titanium dioxide
The preparation method of silicon, including:
After silica slurry is frozen into solid, carries out vacuum lyophilization, obtain silicon-dioxide powdery, then by dioxy
SiClx powder body is heated to 130～180 DEG C, stirs and adds silazane, obtains super insulating material silicon dioxide.
The beneficial effects of the present invention is: use cryodesiccated mode, make the filter cake of the silicon dioxide of synthesis, through supercool
It is frozen into solid, at low temperatures evacuation, obtains water in making silicon dioxide micropore and directly risen Huawei's vaporous water by solid, vaporous water is taken off
Remove, be by ice distillation dehydration during due to removing water, there is not the surface tension of water, make super insulating material silicon dioxide be dried
Time nanometer micropore do not cave in, there is good insulation effect；Use silazane that silica product is carried out surface modification, obtain
Hydrophobic silicon dioxide, solves the phenomenon of nanometer micropore silicon dioxide water suction.
Detailed description of the invention
By describing the technology contents of the present invention in detail, being realized purpose and effect, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is: use cryodesiccated mode, makes the filter cake of the silicon dioxide of synthesis, passes through
It is frozen into solid, at low temperatures evacuation, obtains water in making silicon dioxide micropore and directly risen Huawei's vaporous water by solid, vaporous water
Removing.By ice distillation dehydration during this method removing water, there is not the surface tension of water, make super insulating material silicon dioxide do
Time dry, nanometer micropore does not caves in, and has good insulation effect.
The present invention provides the preparation method of a kind of super insulating material silicon dioxide, including:
After silica slurry is frozen into solid, carries out vacuum lyophilization, obtain silicon-dioxide powdery, then by dioxy
SiClx powder body is heated to 130～180 DEG C, stirs and adds silazane, obtains super insulating material silicon dioxide.
Concrete, above-mentioned preparation method particularly as follows:
Step 1, the solid water glass modulus of selected high-quality control 2.5-3.6, are configured to SiO2%:2-8, waterglass cools down
To 5-10 DEG C, the ion of positive resin 001 × 7 obtains silicate solution；
Step 2, it is synthesized, adds a certain amount of sodium salt and surfactant, and it is molten to flow addition silicic acid and ammonia, ammonium salt
Liquid, in reactor, slurry pH value controls 8-10, and flows reaction 60-120min, is passed through steam and heats up, reaches temperature 85-of reaction
95 DEG C, aging reaction 60-120min, add diluted acid and be acidified to pH value 3-4.Continue ageing 30-60min.
Step 3, put into freezer dryer freezing solid material, carry out evacuation lyophilization.Add silazane,
Make silicon dioxide drainage.
Knowable to foregoing description, the beneficial effects of the present invention is: use cryodesiccated mode, make the titanium dioxide of synthesis
The filter cake of silicon, through being frozen into solid, evacuation at low temperatures, obtain water in making silicon dioxide micropore and directly risen Huawei's gas by solid
State water, removes vaporous water, is by ice distillation dehydration, there is not the surface tension of water, make superthermal insulation material during due to removing water
When material silicon dioxide is dried, nanometer micropore does not caves in, and has good insulation effect；Use silazane to silica product
Carry out surface modification, obtain hydrophobic silicon dioxide, solve the phenomenon of nanometer micropore silicon dioxide water suction.
Further, weight ratio when silicon-dioxide powdery mixes with silazane is 10～20: 1.
Further, also comprise the steps:
Step 1, by SiO2Mass fraction be 2～8% waterglass be cooled to 5～10 DEG C, cross positive resin ion exchange column
After silicate solution；
Step 2, in pure water, add surfactant, silicate solution, ammonia and ammonium salt solution react, and control reaction
The pH value of system is 8～10, after reaction 60～120min, is warming up to 85～95 DEG C, continues reaction 60～120min, then will be anti-
Answer system pH to be adjusted to 3～4, continue reaction 30～60min；
Step 3, by step 2 gains washing to filter electrical conductivity of water ＜ 50 μ S/cm, after slurrying, defibrination described two
Silicon oxide slurry.
Further, described surfactant is selected from dodecylbenzene sodium sulfonate, ethylene glycol, triethanolamine soap, poly-Pyrusussuriensis
One or more of ester.
Seen from the above description, the structural strength of nanometer micropore silicon dioxide micropore is the most relatively low, and the present invention uses ammonification
Water, ammonium salt are aging under weak base, allow silicon dioxide precursor small particles dissolve and increase big particle, strengthen silicon dioxide skeleton,
Improve the intensity of particle network structure.
Nano particles of silicon dioxide size is uneven, the pore-size distribution width of the silicon dioxide micropore of formation, and the present invention selectes
Relatively low modulus waterglass, controls the degree of polymerization of waterglass, changes the chain length of silicon dioxide, and the sodium silicate of low concentration is at low temperatures
By positive resin, carry out ion exchange, form silicate solution, carrying out and flowing in addition ammonia, ammonium salt and reaction, temperature reaction
And under alkalescence hot conditions, generating uniform pore size size, pore-size distribution is concentrated.
Embodiment 1
Waterglass be formulated as modulus 2.5, SiO2Mass fraction be 3%, the waterglass prepared is beaten by centrifugal pump
To waterglass head tank, water-cooling screw rod formula cooling-water machine is utilized by tubular heat exchanger, waterglass to be cooled to 5 DEG C, with 2m3/ h leads to
Cross the ion exchange column filling positive resin 001 × 7, collect and obtain silicate solution, stand-by.At 10m3In enamel reaction still, first add
Enter 4m3Pure water, adds 5kg PEG4000 surfactant, and flows addition silicic acid and 25% ammonia spirit, slurry pH in reactor
Value controls 8-10, and flows reaction 120min, is passed through steam and heats up, and reaches the temperature 90 DEG C of reaction, aging reaction 60min, adds
It is 3 that diluted acid is acidified to pH value.Continue ageing 60min.Sheet frame material feeding is washed, and first with the tap water washing after filtration, then uses pure water
Washing, to filter electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination, squeezes into slurry storage tank.Slurry loads in square plate, puts into and freezes storehouse and enter
Row is frozen into solid, controls solid thickness at about 2cm.Freezer dryer pre-cooling, puts into freeze solid material freezing dry
In dry machine, unlatching vacuum pump, to drying machine evacuation, vacuum ＜ 50Pa, is dried 24 hours, when material becomes powder completely
Powder, moisture removes the most completely.Take the powder body 200Kg after lyophilization and add 5m3In enamel reaction still, open stirring, logical
In crossing chuck, conduction oil is to powder body heat temperature raising 180 DEG C, and 10Kg hexamethyldisiloxane is slowly added to, with silicon on silicon dioxide
Hydroxyl reacts, organic group replace silicone hydroxyl be connected on silicon dioxide, make silicon dioxide drainage, obtain super absolutely
Hot material silicon dioxide finished product sample one.
Embodiment 2
Waterglass be formulated as modulus 2.8, SiO2Mass fraction be 5%, the waterglass prepared is beaten by centrifugal pump
To waterglass head tank, water-cooling screw rod formula cooling-water machine is utilized by tubular heat exchanger, waterglass to be cooled to 10 DEG C, with 1m3/ h leads to
Cross the ion exchange column filling positive resin 001 × 7, collect and obtain silicate solution, stand-by.At 10m3In enamel reaction still, first add
Enter 4m3Pure water, adds 5Kg lauryl sodium sulfate surfactant, and flows addition silicic acid and 15% ammonia spirit, in reactor
Slurry pH value control 8-10, and flow reaction 90min, be passed through steam heat up, reach reaction temperature 88 DEG C, aging reaction 90min,
Add diluted acid and be acidified to pH value 4.Continue ageing 30min.Sheet frame material feeding is washed, first with the tap water washing after filtration, then with pure
Water washing, to filter electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination, squeezes into slurry storage tank.Slurry loads in square plate, puts into and freezes storehouse
Carry out being frozen into solid, control solid thickness at about 1cm.Freezer dryer pre-cooling, puts into freezing freezing solid material
In drying machine, unlatching vacuum pump, to drying machine evacuation, vacuum ＜ 50Pa, is dried 12 hours, when material becomes completely
Powder, moisture removes the most completely.Take the powder body 250Kg after lyophilization and add 5m3In enamel reaction still, open stirring,
By conduction oil in chuck to powder body heat temperature raising 150 DEG C, 15Kg aminomethoxy silane is slowly added to, and on silicon dioxide
Silicone hydroxyl reacts, and organic group is replaced silicone hydroxyl and is connected on silicon dioxide, make silicon dioxide drainage, obtain super
Adiabator silicon dioxide finished product sample 2.
Embodiment 3
Waterglass be formulated as modulus 2.5, SiO2Mass fraction be 6%, the waterglass prepared is beaten by centrifugal pump
To waterglass head tank, water-cooling screw rod formula cooling-water machine is utilized by tubular heat exchanger, waterglass to be cooled to 10 DEG C, with 1m3/ h leads to
Cross the ion exchange column filling positive resin 001 × 7, collect and obtain silicate solution, stand-by.At 10m3In enamel reaction still, first add
Enter 5m3Pure water, adds 5Kg ethylene glycol surfactant, and flows addition silicic acid and 25% ammonia spirit, slurry pH value in reactor
Control 8-10, and flow reaction 60min, be passed through steam and heat up, reach the temperature 92 DEG C of reaction, aging reaction 120min, add dilute
Acid is acidified to pH value 4.Continue ageing 30min.Sheet frame material feeding is washed, and first with the tap water washing after filtration, then uses pure water
To filter electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination, squeeze into slurry storage tank.Slurry loads in square plate, puts into and freezes storehouse and carry out cold
It is frozen into solid, controls solid thickness at about 1cm.Freezer dryer pre-cooling, puts into freezer dryer freezing solid material
In, unlatching vacuum pump, to drying machine evacuation, vacuum ＜ 50Pa, is dried 12 hours, when material becomes powder completely,
Moisture removes the most completely.Take the powder body 200Kg after lyophilization and add 5m3In enamel reaction still, open stirring, pass through chuck
Interior conduction oil, to powder body heat temperature raising 150 DEG C, is slowly added to 20Kg methylethoxy base silane, enters with silicone hydroxyl on silicon dioxide
Row reaction, replaces silicone hydroxyl organic group and is connected on silicon dioxide, make silicon dioxide drainage, obtain super insulating material
With silicon dioxide finished product sample three.
Embodiment 4
Waterglass be formulated as modulus 3.0, SiO2Mass fraction be 6%, the waterglass prepared is beaten by centrifugal pump
To waterglass head tank, water-cooling screw rod formula cooling-water machine is utilized by tubular heat exchanger, waterglass to be cooled to 10 DEG C, with 1m3/ h leads to
Cross the ion exchange column filling positive resin 001 × 7, collect and obtain silicate solution, stand-by.At 10m3In enamel reaction still, first add
Enter 5m3Pure water, adds 10Kg ethylene glycol surfactant, and flows addition silicic acid and 15% ammonia spirit, slurry pH in reactor
Value controls 8-10, and flows reaction 60min, is passed through steam and heats up, reaches the temperature 95 DEG C of reaction, aging reaction 90min, add dilute
Acid is acidified to pH value 4.Continue ageing 30min.Sheet frame material feeding is washed, and first with the tap water washing after filtration, then uses pure water
To filter electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination, squeeze into slurry storage tank.Slurry loads in square plate, puts into and freezes storehouse and carry out cold
It is frozen into solid, controls solid thickness at about 1cm.Freezer dryer pre-cooling, puts into freezer dryer freezing solid material
In, unlatching vacuum pump, to drying machine evacuation, vacuum ＜ 50Pa, is dried 12 hours, when material becomes powder completely,
Moisture removes the most completely.Take the powder body 200kg after lyophilization and add 5m3In enamel reaction still, open stirring, pass through chuck
Interior conduction oil, to powder body heat temperature raising 150 DEG C, is slowly added to 10Kg vinyl methoxy silane, with silicone hydroxyl on silicon dioxide
React, organic group is replaced silicone hydroxyl and is connected on silicon dioxide, make silicon dioxide drainage, obtain superthermal insulation material
Material silicon dioxide finished product sample four.
The testing result of embodiment 1～4 gained silicon dioxide finished product is as shown in table 1.
Table 1
Embodiment 5
The preparation method of super insulating material silicon dioxide specifically comprises the following steps that
Step 1, waterglass are prepared
The solid water glass modulus of selected high-quality controls 2.5-3.6, adds reverse osmosis membrane processing in putting into cylinder rotary spherical digester
Water (hereinafter referred to as pure water), is passed through the rotary spherical digester through accurate filter, is forced into 0.6MPa, pressurize 2 hours.Concentrated sodium silicate adds instead
The water that permeable membrane processes, is configured to SiO2The waterglass that mass fraction is 2-8%, store standby.
Step 2, positive resin ion exchange
The waterglass prepared gets to waterglass head tank by centrifugal pump, utilizes water-cooling screw rod formula cooling-water machine to pass through tubulation
Heat exchanger is cooled to 5-10 DEG C waterglass, with 1-3m3/ h is by filling the ion exchange column of positive resin 001 × 7, and collection obtains
Silicate solution, stand-by.
Step 3, synthetic reaction and reaming are aging
At 10m3In enamel reaction still, it is initially charged a certain amount of pure water, adds a certain amount of surfactant, and flow addition silicon
Acid and ammonia, ammonium salt solution, in reactor, slurry pH value controls 8-10, and flows reaction 60-120min, is passed through steam and heats up, reaches
To temperature 85-95 DEG C of reaction, aging reaction 60-120min, add diluted acid and be acidified to pH value 3-4.Continue ageing 30-60min.
Step 4, sheet frame material feeding washing, first with the tap water washing after filtration, then with pure water to filtering electrical conductivity of water
＜ 50 μ S/cm, slurrying, defibrination, squeeze into slurry storage tank.
Step 5, slurry load in square plate, put into and freeze storehouse and carry out being frozen into solid.
Step 6, put into freezer dryer freezing solid material, carry out evacuation lyophilization.
Powder body after step 7, lyophilization adds 5m3In enamel reaction still, by conduction oil in chuck, powder body is heated
Intensification 130-180 DEG C, opens stirring, is slowly added to silazane, reacts with silicone hydroxyl on silicon dioxide, organic group is taken
It is connected on silicon dioxide for silicone hydroxyl, makes silicon dioxide drainage.
In sum, the having the beneficial effects that of preparation method of the super insulating material silicon dioxide that the present invention provides:
Use cryodesiccated mode, make the filter cake of the silicon dioxide of synthesis, through being frozen into solid, evacuation at low temperatures, make two
Obtain water in silicon oxide micropore and directly risen Huawei's vaporous water by solid, vaporous water is removed, be de-by ice distillation during due to removing water
, there is not the surface tension of water in water, when making super insulating material silicon dioxide be dried, nanometer micropore does not caves in, and has good
Insulation effect；Use silazane that silica product is carried out surface modification, obtain hydrophobic silicon dioxide, solve nanometer micropore
The phenomenon of silicon dioxide water suction；The structural strength of nanometer micropore silicon dioxide micropore is the most relatively low, and the present invention uses and adds ammonia, ammonium
Salt is aging under weak base, allows silicon dioxide precursor small particles dissolve and increases big particle, strengthen silicon dioxide skeleton, improves grain
The intensity of sub-network structure；Nano particles of silicon dioxide size is uneven, the pore-size distribution width of the silicon dioxide micropore of formation, this
The selected relatively low modulus waterglass of invention, controls the degree of polymerization of waterglass, changes the chain length of silicon dioxide, the sodium silicate of low concentration
At low temperatures by positive resin, carry out ion exchange, form silicate solution, carrying out and flowing in addition ammonia, ammonium salt and reaction,
Under temperature reaction and alkalescence hot conditions, generating uniform pore size size, pore-size distribution is concentrated.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every utilize this
The equivalents that bright description is made, or directly or indirectly it is used in relevant technical field, the most in like manner it is included in this
In bright scope of patent protection.
Claims (4)
1. the preparation method of a super insulating material silicon dioxide, it is characterised in that including:
After silica slurry is frozen into solid, carries out vacuum lyophilization, obtain silicon-dioxide powdery, then by silicon dioxide
Powder body is heated to 130～180 DEG C, stirs and adds silazane, obtains super insulating material silicon dioxide.
The preparation method of super insulating material silicon dioxide the most according to claim 1, it is characterised in that also include as
Lower step:
Step 1, by SiO2Mass fraction be 2～8% waterglass be cooled to 5～10 DEG C, cross after positive resin ion exchange column to obtain silicon
Acid solution；
Step 2, in pure water, add surfactant, silicate solution, ammonia and ammonium salt solution react, and control reaction system
PH value be 8～10, reaction 60～120min after, be warming up to 85～95 DEG C, continue reaction 60～120min, then by reactant
It is that pH value is adjusted to 3～4, continues reaction 30～60min；
Step 3, by step 2 gains washing to filter electrical conductivity of water ＜ 50 μ S/cm, after slurrying, defibrination described titanium dioxide
Silicon slurry.
The preparation method of super insulating material silicon dioxide the most according to claim 2, it is characterised in that described surface
Activating agent selected from dodecylbenzene sodium sulfonate, ethylene glycol, triethanolamine soap, Polysorbate one or more.
The preparation method of super insulating material silicon dioxide the most according to claim 1, it is characterised in that silicon dioxide
Weight ratio when powder body mixes with silazane is 10～20: 1.
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| CN109179431A (en) * | 2018-09-13 | 2019-01-11 | 安徽山河药用辅料股份有限公司 | A kind of preparation method of high bulk density silica |
| CN110255570A (en) * | 2019-07-02 | 2019-09-20 | 中建材衢州金格兰石英有限公司 | A kind of preparation method of high-purity compound stone sand |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107285780A (en) * | 2017-06-30 | 2017-10-24 | 长兴泓矿炉料有限公司 | A kind of magnesium zirconia block and preparation method thereof |
| CN109179431A (en) * | 2018-09-13 | 2019-01-11 | 安徽山河药用辅料股份有限公司 | A kind of preparation method of high bulk density silica |
| CN110255570A (en) * | 2019-07-02 | 2019-09-20 | 中建材衢州金格兰石英有限公司 | A kind of preparation method of high-purity compound stone sand |
Also Published As
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| CN106185964B (en) | 2018-03-06 |
| CN108314053A (en) | 2018-07-24 |
| CN108314053B (en) | 2020-01-03 |
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